Login In
2015 Volume 34 Issue 10
2016, 34(10): 1473-1478
doi: 10.14102/j.cnki.0254-5861.2011-0793
Abstract:
The molecular electronegativity distance vector (MEDV) was applied to characterize the molecular structures of 30 organophosphorous compounds. Optimum MEDV descriptors were selected by using the variable selection and modeling method based on the prediction (VSMP) technique. The quantitative structure-toxicity relationship (QSTR) model was built for acute toxicity (96h pLC50) of organophosphorous compounds to steelhead. The developed QSTR model with strictly internal and external validations presents relatively high correlation coefficient (R2) of 0.9518, leave-one-out (LOO) cross-validated correlation coefficient (QLOO2) of 0.9355, and leave-many-out (LMO) cross-validated correlation coefficient (QLMO2) of 0.9290. The robustness of the model was confirmed by the y-randomization test (Ryrand2=0.0772 and Qyrand2=-0.5313) and bootstrapping (Rbstr2=0.9502 and Qbstr2=0.9177) method. The result of external validation, QF12=0.9336, QF22=0.9336, QF32=0.9447, rm2=0.8120, and CCC=0.9602, shows that the QSTR model has a high predictive ability.
The molecular electronegativity distance vector (MEDV) was applied to characterize the molecular structures of 30 organophosphorous compounds. Optimum MEDV descriptors were selected by using the variable selection and modeling method based on the prediction (VSMP) technique. The quantitative structure-toxicity relationship (QSTR) model was built for acute toxicity (96h pLC50) of organophosphorous compounds to steelhead. The developed QSTR model with strictly internal and external validations presents relatively high correlation coefficient (R2) of 0.9518, leave-one-out (LOO) cross-validated correlation coefficient (QLOO2) of 0.9355, and leave-many-out (LMO) cross-validated correlation coefficient (QLMO2) of 0.9290. The robustness of the model was confirmed by the y-randomization test (Ryrand2=0.0772 and Qyrand2=-0.5313) and bootstrapping (Rbstr2=0.9502 and Qbstr2=0.9177) method. The result of external validation, QF12=0.9336, QF22=0.9336, QF32=0.9447, rm2=0.8120, and CCC=0.9602, shows that the QSTR model has a high predictive ability.
2016, 34(10): 1479-1486
doi: 10.14102/j.cnki.0254-5861.2011-0721
Abstract:
Two PbII coordination polymers [Pb(oba)(2,2'-bipy)]·1.5H2O (1) and [Pb(oba)(phen)] (2) (H2oba2,4-oxybis(benzoic acid), 2,2'-bipy=2,2'-bipyridine, phen=1,10-phenanthroline) were synthesized by hydrothermal reactions and characterized by single-crystal X-ray diffraction, thermogravimetric analyses, IR spectroscopy and elemental analysis. Structures of compounds 1 and 2 are similar. Compounds 1 and 2 show 1D wavy chains, which are further connected through aromatic π-π stacking interactions to expand into 2D wavelike networks. The crystal structure of 2,4-oxybis(benzoic acid) ligand (3) was obtained, and its full geometry optimization was carried out by using DFT methods at the B3LYP/6-31G(d) level. The calculated data show that the bond distances and bond angles were very close to the experimental data. The values of the frontier orbital energies indicate that this configuration is stable. Moreover, the solid-state fluorescence properties of 1~3 have also been investigated.
Two PbII coordination polymers [Pb(oba)(2,2'-bipy)]·1.5H2O (1) and [Pb(oba)(phen)] (2) (H2oba2,4-oxybis(benzoic acid), 2,2'-bipy=2,2'-bipyridine, phen=1,10-phenanthroline) were synthesized by hydrothermal reactions and characterized by single-crystal X-ray diffraction, thermogravimetric analyses, IR spectroscopy and elemental analysis. Structures of compounds 1 and 2 are similar. Compounds 1 and 2 show 1D wavy chains, which are further connected through aromatic π-π stacking interactions to expand into 2D wavelike networks. The crystal structure of 2,4-oxybis(benzoic acid) ligand (3) was obtained, and its full geometry optimization was carried out by using DFT methods at the B3LYP/6-31G(d) level. The calculated data show that the bond distances and bond angles were very close to the experimental data. The values of the frontier orbital energies indicate that this configuration is stable. Moreover, the solid-state fluorescence properties of 1~3 have also been investigated.
2016, 34(10): 1487-1495
doi: 10.14102/j.cnki.0254-5861.2011-0105
Abstract:
The stable structures and stabilities of AgnH2S (n=1~10) clusters have been calculated using the B3P86-DFT method. The results predicate that the stable geometries of AgnH2S clusters can be got by directly adding the H2S molecule on different sites of Agn clusters. Agn clusters would like to bond with sulfur atom and the H2S molecules are partial to adsorb at the top site in the clusters. After adsorption, the structures of Agn clusters and H2S molecule keep the original structures except Ag9. The binding energy of AgnH2S is distinctly larger than that of pure Agn clusters. The second difference in energy and the HOMO and LUMO gaps of Agn and AgnH2S exhibit an obvious odd-even oscillation, which demonstrate that the stabilities of even-numbered silver clusters are relatively more stable than the neighboring odd-numbered silver clusters. Mulliken population analysis shows that charges always transfer from the H2S molecule to Agn clusters in all clusters.
The stable structures and stabilities of AgnH2S (n=1~10) clusters have been calculated using the B3P86-DFT method. The results predicate that the stable geometries of AgnH2S clusters can be got by directly adding the H2S molecule on different sites of Agn clusters. Agn clusters would like to bond with sulfur atom and the H2S molecules are partial to adsorb at the top site in the clusters. After adsorption, the structures of Agn clusters and H2S molecule keep the original structures except Ag9. The binding energy of AgnH2S is distinctly larger than that of pure Agn clusters. The second difference in energy and the HOMO and LUMO gaps of Agn and AgnH2S exhibit an obvious odd-even oscillation, which demonstrate that the stabilities of even-numbered silver clusters are relatively more stable than the neighboring odd-numbered silver clusters. Mulliken population analysis shows that charges always transfer from the H2S molecule to Agn clusters in all clusters.
2016, 34(10): 1496-1502
doi: 10.14102/j.cnki.0254-5861.2011-0720
Abstract:
The new ligand 2-((pyridin-4-ylmethyl)thio)-5-(quinoline-2-yl)-1,3,4-oxadiazole (L) and AgClO4 produced a new coordination polymer: [(Ag2L2ClO4)ClO4]n (1). The complex has been characterized by single-crystal X-ray diffraction, IR, TGA, PXRD, UV and elemental analysis. Compound 1 crystallizes in triclinic system, space group P1, with a=8.4593(5), b=14.5903(9), c=15.7908(10) Å, α=97.357(5), β=99.116(5), γ=104.470(5)°, V=1834.43(20) Å3, Dc=1.91056 g/cm3, Mr=1055.38, Z=2, F(000)=1048, u=1.399 mm-1, the final S=1.002, R=0.049 and wR=0.105. The compound consists of a double helix chain. The neighboring chains interact via two kinds of π-π interactions to form a two-dimensional (2D) sheet. Each sheet interacts with the neighboring sheets via π-π interactions to form an extended 3D supramolecular network.
The new ligand 2-((pyridin-4-ylmethyl)thio)-5-(quinoline-2-yl)-1,3,4-oxadiazole (L) and AgClO4 produced a new coordination polymer: [(Ag2L2ClO4)ClO4]n (1). The complex has been characterized by single-crystal X-ray diffraction, IR, TGA, PXRD, UV and elemental analysis. Compound 1 crystallizes in triclinic system, space group P1, with a=8.4593(5), b=14.5903(9), c=15.7908(10) Å, α=97.357(5), β=99.116(5), γ=104.470(5)°, V=1834.43(20) Å3, Dc=1.91056 g/cm3, Mr=1055.38, Z=2, F(000)=1048, u=1.399 mm-1, the final S=1.002, R=0.049 and wR=0.105. The compound consists of a double helix chain. The neighboring chains interact via two kinds of π-π interactions to form a two-dimensional (2D) sheet. Each sheet interacts with the neighboring sheets via π-π interactions to form an extended 3D supramolecular network.
2016, 34(10): 1503-1507
doi: 10.14102/j.cnki.0254-5861.2011-0715
Abstract:
A new two-dimensional Pb(II) coordination polymer, [Pb2(L)(tpphz)1.5(NO3)2]·H2O (1), has been obtained by the hydrothermal reaction of tetrapyrido[3,2-a:2',3'-c:3",2"-h:2"',3"'-j]-phenazine (tpphz) and 2,2'-bipyridyl-3,3'-dicarboxylic acid (H2L). It crystallizes in monoclinic, space group P21/c with a=15.344(3), b=14.111(3), c=21.963(4) Å, β=106.89(3)°, V=4550.1(16) Å3, Z=4, C48H26N13O11Pb2, Mr=1375.20, Dc=2.007 g/cm3, F(000)=2628, μ(MoKa)=7.471 mm-1, R=0.0339 and wR=0.0808. In 1, the two crystallographically independent tpphz ligands adopt the same bis-chelating coordination mode, but they play different roles in the structure of 1. One type of tpphz ligands bridge the Pb(II) cations to generate a zigzig chain, where the L anions are located on one side of the chain. Further, adjacent chains are linked by the other type of tpphz ligands into a two-dimensional layer structure. Additionally, the solid state luminescent property of 1 was also studied at room temperature.
A new two-dimensional Pb(II) coordination polymer, [Pb2(L)(tpphz)1.5(NO3)2]·H2O (1), has been obtained by the hydrothermal reaction of tetrapyrido[3,2-a:2',3'-c:3",2"-h:2"',3"'-j]-phenazine (tpphz) and 2,2'-bipyridyl-3,3'-dicarboxylic acid (H2L). It crystallizes in monoclinic, space group P21/c with a=15.344(3), b=14.111(3), c=21.963(4) Å, β=106.89(3)°, V=4550.1(16) Å3, Z=4, C48H26N13O11Pb2, Mr=1375.20, Dc=2.007 g/cm3, F(000)=2628, μ(MoKa)=7.471 mm-1, R=0.0339 and wR=0.0808. In 1, the two crystallographically independent tpphz ligands adopt the same bis-chelating coordination mode, but they play different roles in the structure of 1. One type of tpphz ligands bridge the Pb(II) cations to generate a zigzig chain, where the L anions are located on one side of the chain. Further, adjacent chains are linked by the other type of tpphz ligands into a two-dimensional layer structure. Additionally, the solid state luminescent property of 1 was also studied at room temperature.
2016, 34(10): 1508-1512
doi: 10.14102/j.cnki.0254-5861.2011-0712
Abstract:
A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n (1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [CuN3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data: monoclinic, space group C2/c, a=17.8599(15), b=8.2889(5), c=14.8076(14) Å, β=113.2580(10)°, V=2014.0(3) Å3, Z=8, S=1.025, the final R=0.0303, wR=0.0825 for 1460 observed reflections with I>2σ(I) and R=0.0386, wR=0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.
A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n (1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [CuN3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data: monoclinic, space group C2/c, a=17.8599(15), b=8.2889(5), c=14.8076(14) Å, β=113.2580(10)°, V=2014.0(3) Å3, Z=8, S=1.025, the final R=0.0303, wR=0.0825 for 1460 observed reflections with I>2σ(I) and R=0.0386, wR=0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.
2016, 34(10): 1513-1518
doi: 10.14102/j.cnki.0254-5861.2011-0710
Abstract:
One new coordination polymer, namely {[Zn(HL)(Hbipy)]2·3H2O}n (bipy=4,4'-bipyridine, H4L=6-(3',4'-dicarboxyl-phenoxy) isophthalic acid), has been synthesized through a hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectra (IR), and thermogravimetric (TG) analysis. The crystal structure is of monoclinic, space group P21/n with a=9.6435(3), b=19.8515(7), c=12.9731(5) Å, β=103.023(4)°, V=2419.67(15) Å3, C52H38Zn2N4O21, Mr=1185.6, Z=2, Dc=1.619 g/cm3, F(000)=1200, μ=1.083 mm-1, the final R=0.0443 and wR=0.1079 for 4269 observed reflections (I>2σ(I). The compound features a two-dimensional (2D) framework and stabilizes itself by interlayer π…π interactions and innerlayer hydrogen bonds. The 2D layer presents a simple 3-connected 63 topology. Moreover, the thermal dynamic stability and luminescent property of the compound have also been discussed in detail.
One new coordination polymer, namely {[Zn(HL)(Hbipy)]2·3H2O}n (bipy=4,4'-bipyridine, H4L=6-(3',4'-dicarboxyl-phenoxy) isophthalic acid), has been synthesized through a hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectra (IR), and thermogravimetric (TG) analysis. The crystal structure is of monoclinic, space group P21/n with a=9.6435(3), b=19.8515(7), c=12.9731(5) Å, β=103.023(4)°, V=2419.67(15) Å3, C52H38Zn2N4O21, Mr=1185.6, Z=2, Dc=1.619 g/cm3, F(000)=1200, μ=1.083 mm-1, the final R=0.0443 and wR=0.1079 for 4269 observed reflections (I>2σ(I). The compound features a two-dimensional (2D) framework and stabilizes itself by interlayer π…π interactions and innerlayer hydrogen bonds. The 2D layer presents a simple 3-connected 63 topology. Moreover, the thermal dynamic stability and luminescent property of the compound have also been discussed in detail.
2016, 34(10): 1519-1524
doi: 10.14102/j.cnki.0254-5861.2011-0746
Abstract:
One novel nickel coordination polymer, {[Ni(OTP)(bib)1.5(H2O)]·2H2O}n (1, H2OTP=2-hydroxy-5-(3',5'-terephthalic acid) pyridine, bib=1,4-bis(1-imdazoly)benzene), has been synthesized and characterized by elemental analysis (EA), IR, powder X-ray diffraction (PXRD), and thermogravimetric (TG) analyses. The crystal of 1 crystallizes in monoclinic, space group P21/n with a=12.2860(5), b=13.8246(6), c=19.0140(8) Å, β=104.3870(1)°, V=3128.2(2) Å3, Z=4, C32H28N7NiO8, Mr=697.32, Dc=1.481 g/cm3, F(000)=1444 and µ(MoKα)=0.684 mm-1. The final R=0.0704 and wR=0.1764 for 5485 observed reflections with I>2σ(I) and R=0.1087 and wR=0.2010 for all data. Topology analysis reveals that complex 1 is a 3D 2-fold interpenetrated {44·66}-nov net based on the 1D [Ni(OTP)]n chain and the 2D [Ni2(bib)3]n sql sheet. And the variable-temperature magnetic susceptibility measurements exhibit weak antiferromagnetic coupling interaction.
One novel nickel coordination polymer, {[Ni(OTP)(bib)1.5(H2O)]·2H2O}n (1, H2OTP=2-hydroxy-5-(3',5'-terephthalic acid) pyridine, bib=1,4-bis(1-imdazoly)benzene), has been synthesized and characterized by elemental analysis (EA), IR, powder X-ray diffraction (PXRD), and thermogravimetric (TG) analyses. The crystal of 1 crystallizes in monoclinic, space group P21/n with a=12.2860(5), b=13.8246(6), c=19.0140(8) Å, β=104.3870(1)°, V=3128.2(2) Å3, Z=4, C32H28N7NiO8, Mr=697.32, Dc=1.481 g/cm3, F(000)=1444 and µ(MoKα)=0.684 mm-1. The final R=0.0704 and wR=0.1764 for 5485 observed reflections with I>2σ(I) and R=0.1087 and wR=0.2010 for all data. Topology analysis reveals that complex 1 is a 3D 2-fold interpenetrated {44·66}-nov net based on the 1D [Ni(OTP)]n chain and the 2D [Ni2(bib)3]n sql sheet. And the variable-temperature magnetic susceptibility measurements exhibit weak antiferromagnetic coupling interaction.
2016, 34(10): 1525-1532
doi: 10.14102/j.cnki.0254-5861.2011-0742
Abstract:
Assembly of Cd(II) nitrate with a new dipyridyltriazole building block 3-(2-pyridyl)-5-(3'-pyridyl)-1H-1,2,4-triazole (2,3'-Hbpt) and benzoic acid (Hba) yields a new coordination compound [Cd(2,3'-bpt)(ba)(H2O)] which was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, TGA and XRPD analysis. Single-crystal X-ray diffraction analysis indicates that the complex belongs to triclinic system, space group P1 with a=6.8972(6), b=8.8182(7), c=16.0484(1) Å, α=75.6330(1), β=85.294(2), γ=69.3450(1)°, V=884.76(13) Å3, Z=2, Dc=1.778 g/cm3, μ=1.276 mm-1, Mr=473.76, F(000)=472, the final R=0.0380 and wR=0.1054 with I>2σ(I). The Cd(II) ion is coordinated by three N-terminal atoms from two 2,3'-Hbpt ligands as well as three O-terminal atoms from ba-and lattice water forming a distorted octahedral coordinated geometry. With the lattice water as hydrogen bond donor, the structure of the title complex is linked into a 2D layer-hole structure from the 0D motif. Theoretical calculation based on density functional theory (DFT) for the ligand is also employed to explicate the stability of different conformations. Moreover, the complex exhibits strong solid state fluorescent emission at room temperature which indicates that the title complex could be a good candidate for potential photoactive materials.
Assembly of Cd(II) nitrate with a new dipyridyltriazole building block 3-(2-pyridyl)-5-(3'-pyridyl)-1H-1,2,4-triazole (2,3'-Hbpt) and benzoic acid (Hba) yields a new coordination compound [Cd(2,3'-bpt)(ba)(H2O)] which was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, TGA and XRPD analysis. Single-crystal X-ray diffraction analysis indicates that the complex belongs to triclinic system, space group P1 with a=6.8972(6), b=8.8182(7), c=16.0484(1) Å, α=75.6330(1), β=85.294(2), γ=69.3450(1)°, V=884.76(13) Å3, Z=2, Dc=1.778 g/cm3, μ=1.276 mm-1, Mr=473.76, F(000)=472, the final R=0.0380 and wR=0.1054 with I>2σ(I). The Cd(II) ion is coordinated by three N-terminal atoms from two 2,3'-Hbpt ligands as well as three O-terminal atoms from ba-and lattice water forming a distorted octahedral coordinated geometry. With the lattice water as hydrogen bond donor, the structure of the title complex is linked into a 2D layer-hole structure from the 0D motif. Theoretical calculation based on density functional theory (DFT) for the ligand is also employed to explicate the stability of different conformations. Moreover, the complex exhibits strong solid state fluorescent emission at room temperature which indicates that the title complex could be a good candidate for potential photoactive materials.
2016, 34(10): 1533-1538
doi: 10.14102/j.cnki.0254-5861.2011-0761
Abstract:
The reaction of 1,2-benzenedicarboxylic acid (H2L) with Zn(NO)3·6H2O and selfdesigned 1,2-bis(imidazol-1-ylmethyl)-benzene) (2-bimb) in DMA/H2O results in the formating of double chains ZnII complex, {[Zn2.5(L)2(bimb)(H2O)]·H2O}n (1), which has been characterized by TGA, PXRD and single-crystal X-ray diffraction. Compound 1 crystalizes in monoclinic, space group P1 with a=11.4030(3), b=11.9722(3), c=13.5702(4) Å, α=89.903(3), β=80.692(2), γ=63.999(3)°, C64H56N8O20Zn5, Mr=1584.01, V=1638.15(9) Å3, Z=1, Dc=1.606 g·cm-3, μ=1.885 mm-1, F(000)=806.0, 2.07< θ< 25°, λ(MoKα)=0.71073 Å, T=293(2) K, the final R=0.0439, wR=0.01393 and S=1.057. X-ray diffraction analysis reveals that complex 1 possesses a 2D double-chain structure. In addition, the solid state luminescent property of complex 1, H2L, and 2-bimb at room temperature are also investigated.
The reaction of 1,2-benzenedicarboxylic acid (H2L) with Zn(NO)3·6H2O and selfdesigned 1,2-bis(imidazol-1-ylmethyl)-benzene) (2-bimb) in DMA/H2O results in the formating of double chains ZnII complex, {[Zn2.5(L)2(bimb)(H2O)]·H2O}n (1), which has been characterized by TGA, PXRD and single-crystal X-ray diffraction. Compound 1 crystalizes in monoclinic, space group P1 with a=11.4030(3), b=11.9722(3), c=13.5702(4) Å, α=89.903(3), β=80.692(2), γ=63.999(3)°, C64H56N8O20Zn5, Mr=1584.01, V=1638.15(9) Å3, Z=1, Dc=1.606 g·cm-3, μ=1.885 mm-1, F(000)=806.0, 2.07< θ< 25°, λ(MoKα)=0.71073 Å, T=293(2) K, the final R=0.0439, wR=0.01393 and S=1.057. X-ray diffraction analysis reveals that complex 1 possesses a 2D double-chain structure. In addition, the solid state luminescent property of complex 1, H2L, and 2-bimb at room temperature are also investigated.
2016, 34(10): 1539-1545
doi: 10.14102/j.cnki.0254-5861.2011-0760
Abstract:
One coordination polymer with bifunctional zwitterionic ligand bearing both carboxylate and tetrazolate groups, [Cd(L1)(N3)]n·nH2O (1, L1=1-(carboxylatomethyl)-4-(5-tetrazolato)pyridinium], has been in situ hydrothermally synthesized and structurally characterized. Compound 1 crystallizes in monoclinic with C2/m space group, a=21.8038(17), b=7.6087(6), c=7.8342(6) Å, β=106.166(2)°, V=1248.29(17) Å3, Z=4, Mr=376.62, Dc=2.004 g·cm-3, F(000)=736, μ=1.772 mm-1, Rint=0.0217, S=1.088, the final R=0.0415 and wR=0.1128 for 1020 observed reflections with I>2σ(I). The compound exhibits two-dimensional coordination sheets, in which infinite anionic [Cd(CN4)(N3)(OCO)]n chains with the tricomponent (μ-azide)(μ-tetrazolate)(μ-carboxylate) bridges are cross-linked by cationic 1-methylenepyridinium spacers of the L1 ligand. This compound in the solid state exhibits blue luminescence assignable to intraligand transitions.
One coordination polymer with bifunctional zwitterionic ligand bearing both carboxylate and tetrazolate groups, [Cd(L1)(N3)]n·nH2O (1, L1=1-(carboxylatomethyl)-4-(5-tetrazolato)pyridinium], has been in situ hydrothermally synthesized and structurally characterized. Compound 1 crystallizes in monoclinic with C2/m space group, a=21.8038(17), b=7.6087(6), c=7.8342(6) Å, β=106.166(2)°, V=1248.29(17) Å3, Z=4, Mr=376.62, Dc=2.004 g·cm-3, F(000)=736, μ=1.772 mm-1, Rint=0.0217, S=1.088, the final R=0.0415 and wR=0.1128 for 1020 observed reflections with I>2σ(I). The compound exhibits two-dimensional coordination sheets, in which infinite anionic [Cd(CN4)(N3)(OCO)]n chains with the tricomponent (μ-azide)(μ-tetrazolate)(μ-carboxylate) bridges are cross-linked by cationic 1-methylenepyridinium spacers of the L1 ligand. This compound in the solid state exhibits blue luminescence assignable to intraligand transitions.
2016, 34(10): 1546-1552
doi: 10.14102/j.cnki.0254-5861.2011-0792
Abstract:
Two novel complexes, [Zn(L12-)(L2)] (1) and [Ni(L32-)(L4)·2H2O] (2), have been synthesized by solvothermal reactions in different solvents through mixing the carboxylate ligand, imidazole-containing ligand and the metal salt. Compound 1 crystallizes in monoclinic, space group P21/c with a=9.21400(15), b=18.1172(3), c=15.7669(2) Å, β=91.1769(13)°, C30H26N4O4Zn, Mr=571.92, V=2631.44(7) Å3, Z=4, Dc=1.444 g·cm-3, μ=1.659 mm-1, F(000)=1184, λ(CuKα)=1.54178 Å, the final R=0.048, wR=0.1442 and S=1.139. Compound 2 crystallizes in triclinic, space group P1 with a=7.0664(3), b=9.5265(4), c=12.8861(6) Å, α=74.066(4), β=87.408(3), γ=83.591(3)°, C34H32N6O6S2Ni, Mr=743.49, V=828.83(6) Å3, Z=1, Dc=1.490 g·cm-3, μ=2.490 mm-1, F(000)=386, λ(CuKα)=1.54178 Å, the final R=0.0315, wR=0.0861 and S=1.022. Complex 1 is the 1D chain which is linked by C-H…O hydrogen bonding interactions to form a 2D supramolecular architecture. Meanwhile, complex 2 is a 2D (4,4) network with the ABCABC stacking mode and then generates a 3D supramolecular architecture through C-H…N and O-H…O hydrogen bonding interactions.
Two novel complexes, [Zn(L12-)(L2)] (1) and [Ni(L32-)(L4)·2H2O] (2), have been synthesized by solvothermal reactions in different solvents through mixing the carboxylate ligand, imidazole-containing ligand and the metal salt. Compound 1 crystallizes in monoclinic, space group P21/c with a=9.21400(15), b=18.1172(3), c=15.7669(2) Å, β=91.1769(13)°, C30H26N4O4Zn, Mr=571.92, V=2631.44(7) Å3, Z=4, Dc=1.444 g·cm-3, μ=1.659 mm-1, F(000)=1184, λ(CuKα)=1.54178 Å, the final R=0.048, wR=0.1442 and S=1.139. Compound 2 crystallizes in triclinic, space group P1 with a=7.0664(3), b=9.5265(4), c=12.8861(6) Å, α=74.066(4), β=87.408(3), γ=83.591(3)°, C34H32N6O6S2Ni, Mr=743.49, V=828.83(6) Å3, Z=1, Dc=1.490 g·cm-3, μ=2.490 mm-1, F(000)=386, λ(CuKα)=1.54178 Å, the final R=0.0315, wR=0.0861 and S=1.022. Complex 1 is the 1D chain which is linked by C-H…O hydrogen bonding interactions to form a 2D supramolecular architecture. Meanwhile, complex 2 is a 2D (4,4) network with the ABCABC stacking mode and then generates a 3D supramolecular architecture through C-H…N and O-H…O hydrogen bonding interactions.
2016, 34(10): 1553-1557
doi: 10.14102/j.cnki.0254-5861.2011-0911
Abstract:
A new dinuclear copper(II) complex [Cu(CH3COO)(C7H5N4)(H2O)]2·3.5H2O has been hydrothermally synthesized with copper acetate, o-acetamidobenzoic acid and 3-(pyridin-2-yl)-1,2,4-triazole. It crystallizes in the monoclinic space group P21/c, with a=12.0188(7), b=13.7993(8), c=8.7488(5) Å, β=101.7350(10)°, V=1420.67(14) Å3, Dc=1.568 g/cm3, Z=1, F(000)=690, the final GOOF=1.145, R=0.0437, and wR=0.1097. The crystal structure shows that the whole molecule consists of two copper ions bridged by two μ2-η1:η0 3-(pyridin-2-yl)-1,2,4-triazole anions. The coordination environment of Cu(II) ion is CuO2N3, giving a distorted square pyramidal geometry. The thermal stability and magnetic properties of the complex were investigated.
A new dinuclear copper(II) complex [Cu(CH3COO)(C7H5N4)(H2O)]2·3.5H2O has been hydrothermally synthesized with copper acetate, o-acetamidobenzoic acid and 3-(pyridin-2-yl)-1,2,4-triazole. It crystallizes in the monoclinic space group P21/c, with a=12.0188(7), b=13.7993(8), c=8.7488(5) Å, β=101.7350(10)°, V=1420.67(14) Å3, Dc=1.568 g/cm3, Z=1, F(000)=690, the final GOOF=1.145, R=0.0437, and wR=0.1097. The crystal structure shows that the whole molecule consists of two copper ions bridged by two μ2-η1:η0 3-(pyridin-2-yl)-1,2,4-triazole anions. The coordination environment of Cu(II) ion is CuO2N3, giving a distorted square pyramidal geometry. The thermal stability and magnetic properties of the complex were investigated.
2016, 34(10): 1558-1564
doi: 10.14102/j.cnki.0254-5861.2011-0681
Abstract:
Hydrothermal reactions of biphenyl-2,3,3',5'-tetracarboxylic acid (H4bptc) with cobalt salt in the presence of 1,4-bis(2-pyridylmethyl)piperazin(bpmp) afforded one novel coordination polymer, namely, [Co(H2bptc)(bpmp)0.5(H2O)]n (1). Its structure was established by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectra and TG analysis. Complex 1 crystallizes in monoclinic, space group P21/c with a=11.4839(11), b=16.6690(16), c=11.5559(11) Å, V=2201.8(4) Å3, Mr=539.35, Dc=1.627 g/cm3, μ(MoKα)=0.841 mm-1, F(000)=1108, Z=4, the final R=0.0309 and wR=0.0705 for 4090 observed reflections (I>2σ(I)). Complex 1 displays a one-dimensional (1D) chain bridged by bpmp. Two carboxylic groups of H4bptc ligand adopt μ1-η1:η1 and μ1-η1:η0 coordination modes to bridge adjacent Co(II) ions together with bpmp ligand to give alternately arranged left-and right-handed helical chains. In addition, variable-temperature magnetic susceptibility measurements indicate that complex 1 shows weak antiferromagnetic interactions between the adjacent Co(II) ions.
Hydrothermal reactions of biphenyl-2,3,3',5'-tetracarboxylic acid (H4bptc) with cobalt salt in the presence of 1,4-bis(2-pyridylmethyl)piperazin(bpmp) afforded one novel coordination polymer, namely, [Co(H2bptc)(bpmp)0.5(H2O)]n (1). Its structure was established by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectra and TG analysis. Complex 1 crystallizes in monoclinic, space group P21/c with a=11.4839(11), b=16.6690(16), c=11.5559(11) Å, V=2201.8(4) Å3, Mr=539.35, Dc=1.627 g/cm3, μ(MoKα)=0.841 mm-1, F(000)=1108, Z=4, the final R=0.0309 and wR=0.0705 for 4090 observed reflections (I>2σ(I)). Complex 1 displays a one-dimensional (1D) chain bridged by bpmp. Two carboxylic groups of H4bptc ligand adopt μ1-η1:η1 and μ1-η1:η0 coordination modes to bridge adjacent Co(II) ions together with bpmp ligand to give alternately arranged left-and right-handed helical chains. In addition, variable-temperature magnetic susceptibility measurements indicate that complex 1 shows weak antiferromagnetic interactions between the adjacent Co(II) ions.
2016, 34(10): 1565-1570
doi: 10.14102/j.cnki.0254-5861.2011-0668
Abstract:
A new CoⅡ coordination complex, namely [Co(iba)(N3)]n, was prepared by the hydrothermal reaction of Co(NO3)2·6H2O with NaN3 in the presence of 4-imidazol-1-yl-benzoic acid (Hiba). Compound 1 crystallizes in orthorhombic, space group Pbca with a=6.782(2), b=19.93(5), c=15.96(4) Å, V=2157.2(3) Å3, Z=8, C10H7O2N5Co, Mr=228.14, Dc=1.774 g/cm3, F(000)=1160, μ(MoKα)=1.592 mm-1. The final R and wR are 0.0706 and 0.1990 for 1160 observed reflections with I>2σ(I). Each iba-coordinates in a bidentate fashion with two CoⅡ ions and every two adjacent CoⅡ ions were connected by one azido ion to form a 3D two-fold interpenetrating framework. Thermogravimeteric analysis (TGA) of compound 1 reveals that the loss of moiety of azido ion occurs from 200 ℃ to about 260 ℃ and the framework begins to decompose above 300 ℃. The magnetic property investigation of compound 1 demonstrates that it displays ferromagnetic coupling between CoⅡ ions.
A new CoⅡ coordination complex, namely [Co(iba)(N3)]n, was prepared by the hydrothermal reaction of Co(NO3)2·6H2O with NaN3 in the presence of 4-imidazol-1-yl-benzoic acid (Hiba). Compound 1 crystallizes in orthorhombic, space group Pbca with a=6.782(2), b=19.93(5), c=15.96(4) Å, V=2157.2(3) Å3, Z=8, C10H7O2N5Co, Mr=228.14, Dc=1.774 g/cm3, F(000)=1160, μ(MoKα)=1.592 mm-1. The final R and wR are 0.0706 and 0.1990 for 1160 observed reflections with I>2σ(I). Each iba-coordinates in a bidentate fashion with two CoⅡ ions and every two adjacent CoⅡ ions were connected by one azido ion to form a 3D two-fold interpenetrating framework. Thermogravimeteric analysis (TGA) of compound 1 reveals that the loss of moiety of azido ion occurs from 200 ℃ to about 260 ℃ and the framework begins to decompose above 300 ℃. The magnetic property investigation of compound 1 demonstrates that it displays ferromagnetic coupling between CoⅡ ions.
2016, 34(10): 1571-1578
doi: 10.14102/j.cnki.0254-5861.2011-0629
Abstract:
Reactions of N,N'-diisopropyl-thiourea (abbreviated as L1) with CuCl2 and CuBr2 afforded the trimeric (L1CuCl)3 (1) and (L1CuBr)3 (2), respectively, featuring the sulfur bridged Cu3S3 six-membered ring each as the core structure. During the reaction, Cu(II) was reduced to Cu(I). Similarly, the reactions of L1 with CuCl and CuBr gave the same products as those by L1 with respective CuCl2 and CuBr2. In contrast, treatment of 1,3-diisopropyl-4,5-dimethylimidazole-2(3H)-thione (L2) with CuI led to the formation of sulfur and iodide mixed-bridged complex [(L2)4(CuI)5] (3), in which two co-vertice Cu3S2I six-membered rings were fused by an iodide atom. Compounds obtained were characterized by 1H NMR and 13C spectroscopy, elemental analysis, and single-crystal X-ray diffraction. 2 belongs to the monoclinic system, space group P21/c with a=19.6009(10), b=11.5069(6), c=17.1744(9) Å, β=109.062(3)°, V=3661.2(3) Å3, C21H48Br3Cu3N6S3, Mr=911.18, Z=4, Dc=1.653 Mg/m3, μ(MoKα)=5.192 mm-1, F(000)=1824, S=1.030, the final R=0.0374 and wR=0.0808 for 4988 observed reflections (I>2σ(I)) and R=0.0726 and wR=0.0916 for all data. 3·2THF belongs to the monoclinic system, space group P21/c with a=19.7335(6), b=13.3544(4), c=29.6355(11) Å, β=105.415(2)°, V=7528.9(4) Å3, C52H96Cu5I5N8O2S4, Mr=1945.81, Z=4, Dc=1.717 Mg/m3, μ(MoKα)=3.589 mm-1, F(000)=3816, S=1.034, the final R=0.0325 and wR=0.0810 for 5704 observed reflections (I>2σ(I)) and R=0.0447 and wR=0.0910 for all data.
Reactions of N,N'-diisopropyl-thiourea (abbreviated as L1) with CuCl2 and CuBr2 afforded the trimeric (L1CuCl)3 (1) and (L1CuBr)3 (2), respectively, featuring the sulfur bridged Cu3S3 six-membered ring each as the core structure. During the reaction, Cu(II) was reduced to Cu(I). Similarly, the reactions of L1 with CuCl and CuBr gave the same products as those by L1 with respective CuCl2 and CuBr2. In contrast, treatment of 1,3-diisopropyl-4,5-dimethylimidazole-2(3H)-thione (L2) with CuI led to the formation of sulfur and iodide mixed-bridged complex [(L2)4(CuI)5] (3), in which two co-vertice Cu3S2I six-membered rings were fused by an iodide atom. Compounds obtained were characterized by 1H NMR and 13C spectroscopy, elemental analysis, and single-crystal X-ray diffraction. 2 belongs to the monoclinic system, space group P21/c with a=19.6009(10), b=11.5069(6), c=17.1744(9) Å, β=109.062(3)°, V=3661.2(3) Å3, C21H48Br3Cu3N6S3, Mr=911.18, Z=4, Dc=1.653 Mg/m3, μ(MoKα)=5.192 mm-1, F(000)=1824, S=1.030, the final R=0.0374 and wR=0.0808 for 4988 observed reflections (I>2σ(I)) and R=0.0726 and wR=0.0916 for all data. 3·2THF belongs to the monoclinic system, space group P21/c with a=19.7335(6), b=13.3544(4), c=29.6355(11) Å, β=105.415(2)°, V=7528.9(4) Å3, C52H96Cu5I5N8O2S4, Mr=1945.81, Z=4, Dc=1.717 Mg/m3, μ(MoKα)=3.589 mm-1, F(000)=3816, S=1.034, the final R=0.0325 and wR=0.0810 for 5704 observed reflections (I>2σ(I)) and R=0.0447 and wR=0.0910 for all data.
2016, 34(10): 1579-1584
doi: 10.14102/j.cnki.0254-5861.2011-0697
Abstract:
A novel coordination polymer {[Zn2(pda)2(bmp)1.5]·2H2O}n (1, H2pda=1,4-phenyl enediacetic acid and bmp=1,4-bis(2-methy limidazol-3-ium-1-yl)biphenyl) was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectroscopy and powder X-ray diffraction (PXRD). Complex {[Zn2(pda)2(bmp)1.5]·2H2O}n (1) is of triclinic system, space group P1 with a=10.132 (5), b=11.854(5), c=18.784(5) Å, α=80.256(5), β=75.163(5), γ=75.620(5)°, Z=2, V=2099.0(15) Å3, Mr=908.54, Dc=1.437 g/cm3, F(000)=938 and µ=1.206 mm-1. The final R=0.0541 and wR=0.1397 for 8017 observed reflections with I>2σ(I). Complex 1 displays a three-dimensional (3D) self-interpenetrated 6-connected topological net with point symbol (48.67). Furthermore, the luminescent property of complex 1 was investigated in the solid state at room temperature.
A novel coordination polymer {[Zn2(pda)2(bmp)1.5]·2H2O}n (1, H2pda=1,4-phenyl enediacetic acid and bmp=1,4-bis(2-methy limidazol-3-ium-1-yl)biphenyl) was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectroscopy and powder X-ray diffraction (PXRD). Complex {[Zn2(pda)2(bmp)1.5]·2H2O}n (1) is of triclinic system, space group P1 with a=10.132 (5), b=11.854(5), c=18.784(5) Å, α=80.256(5), β=75.163(5), γ=75.620(5)°, Z=2, V=2099.0(15) Å3, Mr=908.54, Dc=1.437 g/cm3, F(000)=938 and µ=1.206 mm-1. The final R=0.0541 and wR=0.1397 for 8017 observed reflections with I>2σ(I). Complex 1 displays a three-dimensional (3D) self-interpenetrated 6-connected topological net with point symbol (48.67). Furthermore, the luminescent property of complex 1 was investigated in the solid state at room temperature.
2016, 34(10): 1585-1592
doi: 10.14102/j.cnki.0254-5861.2011-0702
Abstract:
A new compound, {[Sm2L3(H2O)4]·(4,4'-bpy)·3H2O}n (1, H2L=5-(3-pyridyl methoxy) isophthalic acid, 4,4'-bpy=4,4'-dipyridyl), has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a=11.266(2), b=15.530(3), c=16.711(3) Å, α=112.803(3), β=90.526(1), γ=94.006(3)°, V=2686.6(9) Å3, Z=2, Dc=1.727 g/cm3, μ=2.251 mm-1, F(000)=1392, S=0.999, the final R=0.0296 and wR=0.1058. In the title compound, two crystallographically independent Sm3+ cations are bridged by the carboxyl group of L2- ligands to form two different {Sm2} binuclear subunits which are further connected by two distinct L2- ligands to shape a 1D chain, and such 1D chains are linked up to generate a 2D coordination polymer by another crystallographically unique L2- ligand. The thermogravimetric analysis and luminescent property of the title compound were also investigated.
A new compound, {[Sm2L3(H2O)4]·(4,4'-bpy)·3H2O}n (1, H2L=5-(3-pyridyl methoxy) isophthalic acid, 4,4'-bpy=4,4'-dipyridyl), has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a=11.266(2), b=15.530(3), c=16.711(3) Å, α=112.803(3), β=90.526(1), γ=94.006(3)°, V=2686.6(9) Å3, Z=2, Dc=1.727 g/cm3, μ=2.251 mm-1, F(000)=1392, S=0.999, the final R=0.0296 and wR=0.1058. In the title compound, two crystallographically independent Sm3+ cations are bridged by the carboxyl group of L2- ligands to form two different {Sm2} binuclear subunits which are further connected by two distinct L2- ligands to shape a 1D chain, and such 1D chains are linked up to generate a 2D coordination polymer by another crystallographically unique L2- ligand. The thermogravimetric analysis and luminescent property of the title compound were also investigated.
2016, 34(10): 1593-1597
doi: 10.14102/j.cnki.0254-5861.2011-0698
Abstract:
A novel cobalt(II) coordination polymer, [Co(tdc)(bpmp)(H2O)]n (1), was hydrothermally synthesized using 2,5-thiophenedicarboxylate (tdc) and bis(4-pyridylmethyl)piperazine (bpmp) ligand as the organic linkers. X-ray single-crystal diffraction determination reveals that 1 crystallizes in the monoclinic Cc space group, with a=18.836(2), b=5.9540(7), c=20.414(2) Å, β=97.4300(10)°, V=2270.1(5) Å3, Z=4, Mr=515.44, Dc=1.508 Mg/m3, μ=0.890 mm-1, F(000)=1068, the final R=0.0263 and wR=0.0665 for 3714 observed reflections with I>2σ(I). In compound 1, the Co(II) ions are connected by tdc2- anions to form a 1D double chain, and such chains are further linked by bpmp ligands to form a three-dimensional (3D) structure. Topologically, the structure of 1 represents a uninodal 3D dia (66) topology. What's more, powder X-ray diffraction patterns and photocatalytic property for 1 have also been investigated.
A novel cobalt(II) coordination polymer, [Co(tdc)(bpmp)(H2O)]n (1), was hydrothermally synthesized using 2,5-thiophenedicarboxylate (tdc) and bis(4-pyridylmethyl)piperazine (bpmp) ligand as the organic linkers. X-ray single-crystal diffraction determination reveals that 1 crystallizes in the monoclinic Cc space group, with a=18.836(2), b=5.9540(7), c=20.414(2) Å, β=97.4300(10)°, V=2270.1(5) Å3, Z=4, Mr=515.44, Dc=1.508 Mg/m3, μ=0.890 mm-1, F(000)=1068, the final R=0.0263 and wR=0.0665 for 3714 observed reflections with I>2σ(I). In compound 1, the Co(II) ions are connected by tdc2- anions to form a 1D double chain, and such chains are further linked by bpmp ligands to form a three-dimensional (3D) structure. Topologically, the structure of 1 represents a uninodal 3D dia (66) topology. What's more, powder X-ray diffraction patterns and photocatalytic property for 1 have also been investigated.
2016, 34(10): 1598-1605
doi: 10.14102/j.cnki.0254-5861.2011-0796
Abstract:
A new 3d-4f (CuII-CeIII) hetero-metallic compound containing two kinds of ligands, namely [CuII(H2pdc)(phen)(H2O)](H3O)2[CeIII(pdc)3][CuII(phen)CeIII(pdc)3] (1, H2pdc=pyridine-2,6-dicarboxylic acid, phen=1,10-phenanthroline), has been synthesized by an ionothermal method using the ionic liquid 3-butyl-1-methylimidazolium bromide ([Bmim]Br) as solvent, and characterized by elemental analysis, energy-dispersive X-ray spectroscopy (EDS), IR, XPS and single-crystal X-ray diffraction. The structure reveals that 1 belongs to the triclinic system, space group P1 with a=12.044(7), b=14.841(8), c=22.305(13) Å, α=85.802(12), β=85.471(12), γ=89.174(11)°, Z=2, V=3964(4) Å3, Dc=1.804 g·cm-3, F(000)=2140, μ=1.757 mm-1, the final R=0.0734, wR=0.1094 and S=1.013. The compound can be viewed as a two-dimensional layered structure composed by 3d-4f hetero-nuclear anions [Cu(phen)Ce(pdc)3]-, coordination cations [Cu(H2pdc)(phen)(H2O)]2+, coordination anions [Ce(pdc)3]3- and protonated water molecules via hydrogen bonding interactions and π-π stacking. Moreover, the antimicrobial activities of 1 have been also investigated. The results indicated that its inhibitory activity is slightly higher than that of penicillin against Candida albicans.
A new 3d-4f (CuII-CeIII) hetero-metallic compound containing two kinds of ligands, namely [CuII(H2pdc)(phen)(H2O)](H3O)2[CeIII(pdc)3][CuII(phen)CeIII(pdc)3] (1, H2pdc=pyridine-2,6-dicarboxylic acid, phen=1,10-phenanthroline), has been synthesized by an ionothermal method using the ionic liquid 3-butyl-1-methylimidazolium bromide ([Bmim]Br) as solvent, and characterized by elemental analysis, energy-dispersive X-ray spectroscopy (EDS), IR, XPS and single-crystal X-ray diffraction. The structure reveals that 1 belongs to the triclinic system, space group P1 with a=12.044(7), b=14.841(8), c=22.305(13) Å, α=85.802(12), β=85.471(12), γ=89.174(11)°, Z=2, V=3964(4) Å3, Dc=1.804 g·cm-3, F(000)=2140, μ=1.757 mm-1, the final R=0.0734, wR=0.1094 and S=1.013. The compound can be viewed as a two-dimensional layered structure composed by 3d-4f hetero-nuclear anions [Cu(phen)Ce(pdc)3]-, coordination cations [Cu(H2pdc)(phen)(H2O)]2+, coordination anions [Ce(pdc)3]3- and protonated water molecules via hydrogen bonding interactions and π-π stacking. Moreover, the antimicrobial activities of 1 have been also investigated. The results indicated that its inhibitory activity is slightly higher than that of penicillin against Candida albicans.
2016, 34(10): 1606-1611
doi: 10.14102/j.cnki.0254-5861.2011-0483
Abstract:
Three benzopyranocoumarins (OBH, OMH and ODH) were synthesized and characterized via IR, 1H NMR and HRMS. The HB energy in OBH, OMH and ODH was performed with the density functional theory (DFT) [B3LYP/6-31G*] method. The in vitro antibacterial activity of OBH, OMH and ODH against drug-sensitive S. aureus (S. aureus ATCC 29213) strain, MRSA strain (MRSA XJ 75302), drug-sensitive S. epidermidis strain (S. epidermidis ATCC 14990) and methicillin-resistant S. epidermidis strain (MRSE XJ 75284) was evaluated by observing the minimum inhibitory concentration. The results showed that among the three compounds, ODH exhibited the most potent antibacterial activity.
Three benzopyranocoumarins (OBH, OMH and ODH) were synthesized and characterized via IR, 1H NMR and HRMS. The HB energy in OBH, OMH and ODH was performed with the density functional theory (DFT) [B3LYP/6-31G*] method. The in vitro antibacterial activity of OBH, OMH and ODH against drug-sensitive S. aureus (S. aureus ATCC 29213) strain, MRSA strain (MRSA XJ 75302), drug-sensitive S. epidermidis strain (S. epidermidis ATCC 14990) and methicillin-resistant S. epidermidis strain (MRSE XJ 75284) was evaluated by observing the minimum inhibitory concentration. The results showed that among the three compounds, ODH exhibited the most potent antibacterial activity.
A 2D Cobalt(II) Coordination Polymer [Co(iqnc)2]n: Synthesis, Crystal Structure and Characterization
2016, 34(10): 1612-1616
doi: 10.14102/j.cnki.0254-5861.2011-0708
Abstract:
A new cobalt(II) coordination polymer with the formula of [Co(iqnc)2]n (1, iqnc=l-isoquinolinecarboxylate) has been synthesized through hydrothermal synthesis and structurally characterized by single-crystal X-ray diffraction method. The title coordination polymer represents a two-dimensional layer structure featuring adjacent one-dimensional [Co(iqnc)2]n chains connected with each other by uncoordinated oxygen atoms of carboxylate. Crystal data: monoclinic, space group P21/c, a=15.4302(2), b=5.6743(7), c=9.2307(1) Å, β=98.459(2)°, V=799.41(2) Å3, Z=2, S=1.019, the final R=0.0346, wR=0.0876 (I>2σ(I)) and R=0.0477 and wR=0.1159 for all reflections. In addition, elemental analysis, IR, and magnetism properties are presented.
A new cobalt(II) coordination polymer with the formula of [Co(iqnc)2]n (1, iqnc=l-isoquinolinecarboxylate) has been synthesized through hydrothermal synthesis and structurally characterized by single-crystal X-ray diffraction method. The title coordination polymer represents a two-dimensional layer structure featuring adjacent one-dimensional [Co(iqnc)2]n chains connected with each other by uncoordinated oxygen atoms of carboxylate. Crystal data: monoclinic, space group P21/c, a=15.4302(2), b=5.6743(7), c=9.2307(1) Å, β=98.459(2)°, V=799.41(2) Å3, Z=2, S=1.019, the final R=0.0346, wR=0.0876 (I>2σ(I)) and R=0.0477 and wR=0.1159 for all reflections. In addition, elemental analysis, IR, and magnetism properties are presented.
2016, 34(10): 1617-1625
doi: 10.14102/j.cnki.0254-5861.2011-0713
Abstract:
Two new isostructural multi-metal beryllium borates, M3LiNa4Be4B10O24F (M=Sr (1), Cd (2)), have been synthesized by spontaneous crystallization. The structures were verified by single-crystal X-ray crystallography. The compounds crystallize in the trigonal space group R3, with a=b=9.4645(1) Å, c=38.842(8) Å, V=3013.2(6) Å3, Z=6, F(000)=2568, Dc=3.005 g/cm3, Mr=908.9, R=0.0327, wR=0.0678, μ=8.160 mm-1 for Sr3LiNa4Be4B10O24F and a=b=9.3019(8) Å, c=37.782(7) Å, V=2831.12(9) Å3, Z=6, F(000)=2748, Dc=3.459 g/cm3, Mr=983.24, R=0.0158, wR=0.0455, μ=3.586 mm-1 for Cd3LiNa4Be4B10O24F. The structures are characterized by an infinite two-dimensional [Be8B16O40F2]∞ double layer bridged by [B12O24] groups like a sandwich structure, while the cations reside in tunnels along different directions. UV-vis-IR diffuse reflectance spectroscopy demonstrates that their cut-off edges are below 200 nm. Thermal analysis shows that they melt incongruently and their melting points are around 740~770 ℃.
Two new isostructural multi-metal beryllium borates, M3LiNa4Be4B10O24F (M=Sr (1), Cd (2)), have been synthesized by spontaneous crystallization. The structures were verified by single-crystal X-ray crystallography. The compounds crystallize in the trigonal space group R3, with a=b=9.4645(1) Å, c=38.842(8) Å, V=3013.2(6) Å3, Z=6, F(000)=2568, Dc=3.005 g/cm3, Mr=908.9, R=0.0327, wR=0.0678, μ=8.160 mm-1 for Sr3LiNa4Be4B10O24F and a=b=9.3019(8) Å, c=37.782(7) Å, V=2831.12(9) Å3, Z=6, F(000)=2748, Dc=3.459 g/cm3, Mr=983.24, R=0.0158, wR=0.0455, μ=3.586 mm-1 for Cd3LiNa4Be4B10O24F. The structures are characterized by an infinite two-dimensional [Be8B16O40F2]∞ double layer bridged by [B12O24] groups like a sandwich structure, while the cations reside in tunnels along different directions. UV-vis-IR diffuse reflectance spectroscopy demonstrates that their cut-off edges are below 200 nm. Thermal analysis shows that they melt incongruently and their melting points are around 740~770 ℃.
